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Method for preparing synthetic terephthalic acid-1,3-trimethylene glycol ester

A technology of polyterephthalic acid and dimethyl phthalate, applied in the field of synthetic polyterephthalic acid 1, to overcome the effects of long synthesis time, poor light stability and shortened reaction time

Active Publication Date: 2010-09-29
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of high-efficiency composite catalyst, which can be used for esterification or transesterification and polycondensation catalysis at the same time through good synergistic effect in the catalytic synthesis of PTT, so as to overcome the easy hydrolysis of titanate itself and its activity in the reaction. Affected by the shortcomings of longer synthesis time, improve the efficiency of synthesis reaction, and make the operation easier

Method used

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  • Method for preparing synthetic terephthalic acid-1,3-trimethylene glycol ester

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Preparation of Catalyst A

[0022] In a reactor equipped with a stirrer and a thermometer, add 100g of 1,3-propanediol, add 1.5g of germanium oxide, add 3.0g of cobalt acetate tetrahydrate, slowly add n-tetrabutyl titanate into the reactor while stirring 3.75 g of ester was stirred for 30 min to obtain a mixed solution. Called Catalyst A.

[0023] 1000 grams of purified terephthalic acid (PTA), 650 grams of 1,3-propylene glycol (1,3-PDO) and an appropriate amount of catalyst A are mixed into a slurry and added to the polymerization kettle (wherein the content of the catalyst in the PTA weight is : Tetrabutyl titanate is 375ppm, cobalt acetate tetrahydrate is 300ppm, germanium oxide is 150ppm), carry out esterification reaction, the pressure is 0.2MPa, the esterification temperature is 230-250 ℃, the by-product is distilled out in the reaction kettle When the amount of product water reaches the theoretical water output, the pressure in the kettle returns to normal pres...

Embodiment 2

[0025] Preparation of Catalyst B

[0026] In a beaker, add 100g of 1,3-propanediol, add 2.5g of germanium oxide, add 1.5g of cobalt phosphate, add 2.0g of tetraisopropyl titanate, place in an ultrasonic system for mixing for 15min, and heat to 70°C at the same time to obtain Homogenous mixture. Call it Catalyst B.

[0027] Preparation of polyester

[0028] Polyester was prepared by the same method as in Example 1, using catalyst B as the reaction catalyst, wherein the content of the catalyst in the mass of PTA was: 200ppm tetraisopropyl titanate, 150ppm cobalt phosphate, and 250ppm germanium oxide.

Embodiment 3

[0030] Preparation of Catalyst C

[0031] Catalyst D was prepared by the preparation method of catalyst A, adding 100g of 1,3-propanediol, adding 1.0g of germanium oxide, adding 1.0g of cobalt nitrate, adding 3.0g of tetrapropyl titanate, heating to 80°C at the same time, and stirring for 60min to obtain a uniform Mixture. Called Catalyst C.

[0032] Preparation of polyester

[0033] Polyester was prepared by the same method as in Example 1, using catalyst C as the reaction catalyst, wherein the content of the catalyst in the mass of PTA was: 300ppm tetrapropyl titanate, 100ppm cobalt nitrate, and 100ppm germanium oxide.

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Abstract

The invention relates to a preparation process for synthesizing polyethylene terephthalate 1, 3- terephthalate catalyst, which comprises adding titanic acid ester, germanium compounds and cobalt compound into liquid dispersed phase of organic solution, wherein the total weight concentration is 4-10%, and preparing the catalyst through mechanical stirring or ultrasonic wave mixed ligand for 10-60 minutes in 0-120 DEG C, wherein the adding content of titanic acid ester, germanium compounds and cobalt compound are respectively 200-500ppm, 50-300ppm and 100-400ppm of reaction monomer mass of terephthalic acid or dimethyl terephthalate. The catalyst is used to prepare PTT products, shortens the esterification and polycondensation reaction times about 30-60min relative to merely using butyl titanate, and the product property viscosity number is 0.70-1.05dL / g, hue b value is kept within 2-6, and slices can be used to process novel synthesis fiber and engineering plastic products.

Description

Technical field: [0001] The present invention relates to a kind of catalyzing terephthalic acid (PTA) or dimethyl terephthalate (DMT) and 1,3-propanediol (1,3-PDO) to carry out esterification or transesterification and polycondensation double function A method for preparing a synthetic poly(trimethylene terephthalate) (PTT) catalyst. Background technique: [0002] Polypropylene terephthalate (PTT) is a new type of polymer material. In addition to the excellent chemical properties of PET fibers, it also has excellent elastic recovery. The rebound rate of PTT fibers is better than that of PET, PBT and PP fibers are comparable to PA. PTT products have many potential uses and broad market application prospects, and it has positive significance for adjusting the product structure of synthetic fibers, adding new varieties, and improving the product grade of synthetic fibers. [0003] At present, various companies at home and abroad are conducting research on the PTT synthesis pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85
Inventor 邹妍朱景利史君李连斌陈颖任建平马城华战怀英朱淑清
Owner PETROCHINA CO LTD
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